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Polyglycerol-10 and preparation method thereof

A technology of polyglycerol and glycerin, applied in the field of polyglycerol-10 and its preparation, can solve the problems of short reaction time, high reaction temperature, many side reactions, etc., and achieve the effects of being beneficial to industrial production and high yield

Inactive Publication Date: 2017-10-10
GUANGDONG HEJI BIOTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When acid is used as a catalyst, the reaction temperature is low, but there are problems such as long reaction time and the need to react under vacuum conditions, deep color of the product, high requirements for equipment, and many side reactions.
The advantages of preparing polyglycerol by alkali catalysis are that the method is mature, the raw materials are sufficient, the price is relatively low, the reaction time is short, and the requirements for equipment are low. Disadvantages such as high degree of polymerization polyglycerin
According to the current domestic reports on polyglycerol literature, it is impossible to realize the industrial production of polyglycerol-10. At the same time, the degree of polymerization of polyglycerol in the domestic market is relatively low, and it is relatively dispersed. Generally, it is an oligomerization component of less than 5 polyglycerols.

Method used

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  • Polyglycerol-10 and preparation method thereof
  • Polyglycerol-10 and preparation method thereof

Examples

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preparation example Construction

[0012] One aspect of the present invention provides a method for preparing polyglycerol-10, the method comprising:

[0013] (1) In the presence of an acid catalyst, glycerol and glycidol are polymerized to obtain a polyglycerol crude product,

[0014] (2) neutralize the product of the polymerization reaction, and use molecular distillation equipment to distill the neutralized product, and the resulting heavy component is polyglycerol-10;

[0015] Wherein, the condensation surface of heavy components set by the molecular distillation equipment is above 85°C, the condensation surface of light components is 65-90°C, and the condensation surface of heavy components is higher than that of light components.

[0016] According to the present invention, polyglycerol-10 means a polyglycerol product with an average degree of polymerization of about 10.

[0017] According to the present invention, in step (1), glycidol can be called glycidol again, and its structure is In the present ...

Embodiment 1

[0033] This example is used to illustrate the polyglycerol-10 of the present invention and its preparation method.

[0034] (1) Add glycerin and acid catalyst (see Table 1 for dosage and type) into the container, stir and heat up to 130°C, and keep stirring at constant temperature for 5 minutes; add glycidol (see Table 1 for dosage) dropwise to In the above mixed system, after the dropwise addition (about 15 minutes), keep the temperature of 130°C for 2 hours to obtain a light crystal yellow transparent viscous polyglycerol crude product;

[0035] (2) Heating the crude product of polyglycerol to dissolve, and adding 5% by weight of sodium hydroxide aqueous solution for neutralization, then transferring the crude product to molecular distillation equipment for purification operation, and the temperature setting includes heat preservation surface, evaporation surface and condensation surface (heavy component and heavy component), as shown in Table 1 for details. The heavy compo...

Embodiment 2

[0038] This example is used to illustrate the polyglycerol-10 of the present invention and its preparation method.

[0039] (1) Add glycerin and acid catalyst (see Table 1 for dosage and type) into the container, stir and heat up to 115°C, and continue stirring at constant temperature for 10 minutes; add glycidol (see Table 1 for dosage) dropwise to In the above mixed system, after the dropwise addition (about 15 minutes), keep the temperature of 115°C for 3 hours to obtain a light crystal yellow transparent viscous polyglycerol crude product;

[0040] (2) Heating the crude product of polyglycerol to dissolve, and adding 5% by weight of sodium hydroxide aqueous solution for neutralization, then transferring the crude product to molecular distillation equipment for purification operation, and the temperature setting includes heat preservation surface, evaporation surface and condensation surface (heavy component and heavy component), as shown in Table 1 for details. The heavy ...

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Abstract

The invention relates to the field of polyglycerol synthesis, in particular to polyglycerol-10 and a preparation method thereof. The preparation method of polyglycerol-10 comprises the following steps: (1) a crude polyglycerol product is prepared from glycerol and glycidol through a polymerization reaction in presence of an acid catalyst; (2) the polymerization reaction product is neutralized, a neutralization product is distilled by molecular distillation equipment, and the obtained heavy constituent is polyglycerol-10, wherein the heavy constituent condensing surface set by the molecular distillation equipment is at the temperature of 85 DEG C or higher, the light constituent condensing surface is at the temperature of 65-90 DEG C, and the heavy constituent condensing surface is higher than the light constituent condensing surface. With adoption of the method, the polyglycerol-10 product with higher purity is prepared with high yield by means of molecular distillation, and the method is beneficial to industrial production.

Description

technical field [0001] The invention relates to the field of polyglycerol synthesis, in particular to polyglycerol-10 and a preparation method thereof. Background technique [0002] Polyglycerol is an organic compound of low molecular weight polyether polyols. It has a wide range of uses and can be directly used as a moisturizer, thickener, plasticizer and hydrophilic modifier. Its derivatives, polyglycerol fatty acid Esters are widely used in industries such as food, cosmetics, daily chemicals, medicine and detergents. [0003] At present, the methods for synthesizing polyglycerol in industry mainly include glycerol and non-glycerol methods. Non-glycerin synthesis routes mainly include allyl ether method, glycerin acetonide method, monochloropropanediol and epichlorohydrin method, etc. These raw materials generally need to be carried out under reduced pressure during the reaction, and the operation steps are cumbersome, and there are many by-products produced. The crude p...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C41/42C07C43/13
CPCC07C41/03C07C41/42C07C43/135
Inventor 何廷刚张炽坚陆锦平黎伟杰卢永杰江桦
Owner GUANGDONG HEJI BIOTECH CO LTD
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